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Water → 4-(4-(3-(2-methoxy-5-(trifluoromethyl)phenyl)ureido)phenoxy)-N-methylpicolinamide

HRID 78331
ノート
印刷プレビュー

反応式

HRID 78331 の反応式
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][C:4]=1[NH2:5].C1N=CN([C:19](N2C=NC=C2)=[O:20])C=1.[CH3:26][NH:27][C:28]([C:30]1[CH:35]=[C:34]([O:36][C:37]2[CH:43]=[CH:42][C:40]([NH2:41])=[CH:39][CH:38]=2)[CH:33]=[CH:32][N:31]=1)=[O:29].O>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:9]=[CH:8][C:7]([C:10]([F:11])([F:12])[F:13])=[CH:6][C:4]=1[NH:5][C:19]([NH:41][C:40]1[CH:42]=[CH:43][C:37]([O:36][C:34]2[CH:33]=[CH:32][N:31]=[C:30]([C:28](=[O:29])[NH:27][CH3:26])[CH:35]=2)=[CH:38][CH:39]=1)=[O:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 682631,1'-CarbonyldiimidazoleHCID 6006372-Methoxy-5-(trifluoromethyl)anilineHCID 166551294-(4-Aminophenoxy)-N-methylpicolinamide

生成物 1

HCID 101276604-(4-(3-(2-methoxy-5-(trifluoromethyl)phenyl)ureido)phenoxy)-N-methylpicolinamide収率 30%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

To a solution of 2-methoxy-5-(trifluoromethyl)aniline (0.15 g) in anh CH2Cl2 (15 mL) at 0° C. was added CDI (0.13 g). The resulting solution was allowed to warm to room temp. over 1 h, was stirred at room temp. for 16 h, then was treated with 4-(2-(N-methylcarbamoyl)-4-pyridyloxy)aniline (0.18 g). The resulting yellow solution was stirred at room temp. for 72 h, then was treated with H2O (125 mL). The resulting aqueous mixture was extracted with EtOAc (2×150 mL). The combined organics were washed with a saturated NaCl solution (100 mL), dried (MgSO4) and concentrated under reduced pressure. The residue was triturated (90% EtOAc/10% hexane). The resulting white solids were collected by filtration and washed with EtOAc. The filtrate was concentrated under reduced pressure and the residual oil purified by column chromatography (gradient from 33% EtOAc/67% hexane to 50% EtOAc/50% hexane to 100% EtOAc) to give N-(2-methoxy-5-(trifluoromethyl)phenyl)-N′-(4-(2-(N-methylcarbamoyl)-4-pyridyloxy)phenyl)urea as a light tan solid (0.098 g, 30%): TLC (100% EtOAc) Rf 0.62; 1H NMR (DMSO-d6) δ 2.76 (d, J=4.8 Hz, 3H), 3.96 (s, 3H), 7.1-7.6 and 8.4-8.6 (m, 11H), 8.75 (d, J=4.8 Hz, 1H), 9.55 (s, 1H); FAB-MS m/z 461 ((M+H)+).

後処理

  1. temperatureto warm to room temp. over 1 h
  2. stirringThe resulting yellow solution was stirred at room temp. for 72 h
  3. extractionThe resulting aqueous mixture was extracted with EtOAc (2×150 mL)
  4. washThe combined organics were washed with a saturated NaCl solution (100 mL)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was triturated (90% EtOAc/10% hexane)
  8. filtrationThe resulting white solids were collected by filtration
  9. washwashed with EtOAc
  10. concentrationThe filtrate was concentrated under reduced pressure
  11. customthe residual oil purified by column chromatography (gradient from 33% EtOAc/67% hexane to 50% EtOAc/50% hexane to 100% EtOAc)

出典と根拠

ORDレコード
ord-2857cc8ccf7b47feab4e812313b967b6
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08841330B2

反応ノート

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